CN104891534B - A kind of method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide - Google Patents
A kind of method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide Download PDFInfo
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- CN104891534B CN104891534B CN201510316496.8A CN201510316496A CN104891534B CN 104891534 B CN104891534 B CN 104891534B CN 201510316496 A CN201510316496 A CN 201510316496A CN 104891534 B CN104891534 B CN 104891534B
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- magnesium hydroxide
- purity
- calcic
- activity
- magnesium
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 134
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 131
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 131
- 238000000034 method Methods 0.000 title claims abstract description 60
- 230000000694 effects Effects 0.000 title claims abstract description 33
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000007864 aqueous solution Substances 0.000 claims abstract description 22
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011575 calcium Substances 0.000 claims abstract description 21
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 27
- 239000000725 suspension Substances 0.000 claims description 21
- 239000011164 primary particle Substances 0.000 claims description 19
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 12
- 239000011777 magnesium Substances 0.000 claims description 12
- 229910052749 magnesium Inorganic materials 0.000 claims description 12
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 10
- 235000011147 magnesium chloride Nutrition 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000001103 potassium chloride Substances 0.000 claims description 5
- 235000011164 potassium chloride Nutrition 0.000 claims description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 229960001484 edetic acid Drugs 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- DZCAZXAJPZCSCU-UHFFFAOYSA-K sodium nitrilotriacetate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC([O-])=O DZCAZXAJPZCSCU-UHFFFAOYSA-K 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- KQTIIICEAUMSDG-UHFFFAOYSA-N tricarballylic acid Chemical compound OC(=O)CC(C(O)=O)CC(O)=O KQTIIICEAUMSDG-UHFFFAOYSA-N 0.000 claims description 4
- WUOACPNHFRMFPN-VIFPVBQESA-N (R)-(+)-alpha-terpineol Chemical compound CC1=CC[C@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-VIFPVBQESA-N 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- RWLDAJMGAVDXSH-UHFFFAOYSA-N ethane-1,1,2-tricarboxylic acid Chemical compound OC(=O)CC(C(O)=O)C(O)=O RWLDAJMGAVDXSH-UHFFFAOYSA-N 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical group OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- AYAUBWSUZRFVQO-UHFFFAOYSA-N 2-[2-(4-phenyl-5-sulfanylidene-1h-1,2,4-triazol-3-yl)ethyl]benzo[de]isoquinoline-1,3-dione Chemical compound O=C1C(C=23)=CC=CC3=CC=CC=2C(=O)N1CCC1=NNC(=S)N1C1=CC=CC=C1 AYAUBWSUZRFVQO-UHFFFAOYSA-N 0.000 claims 1
- 244000248349 Citrus limon Species 0.000 claims 1
- 235000005979 Citrus limon Nutrition 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 125000001309 chloro group Chemical group Cl* 0.000 claims 1
- 235000015424 sodium Nutrition 0.000 claims 1
- 239000000395 magnesium oxide Substances 0.000 abstract description 30
- 239000000126 substance Substances 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 239000003063 flame retardant Substances 0.000 abstract description 10
- 239000007791 liquid phase Substances 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 239000003463 adsorbent Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000006477 desulfuration reaction Methods 0.000 abstract description 3
- 230000023556 desulfurization Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000004913 activation Effects 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 235000012254 magnesium hydroxide Nutrition 0.000 description 111
- 239000000047 product Substances 0.000 description 27
- 238000001914 filtration Methods 0.000 description 18
- 238000003756 stirring Methods 0.000 description 16
- 238000005406 washing Methods 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 235000002639 sodium chloride Nutrition 0.000 description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 10
- 239000012535 impurity Substances 0.000 description 9
- 238000010792 warming Methods 0.000 description 9
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 8
- 239000001095 magnesium carbonate Substances 0.000 description 8
- 235000014380 magnesium carbonate Nutrition 0.000 description 8
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 6
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- 241001131796 Botaurus stellaris Species 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 4
- 235000011941 Tilia x europaea Nutrition 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 4
- 235000015165 citric acid Nutrition 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000004571 lime Substances 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 235000011116 calcium hydroxide Nutrition 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 229940083608 sodium hydroxide Drugs 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- -1 but often calcic Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000010423 industrial mineral Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- 241000721047 Danaus plexippus Species 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 1
- BYCMGBGNQBDTCB-UHFFFAOYSA-I [OH-].[Mg+2].[Ce+3].[OH-].[OH-].[OH-].[OH-] Chemical compound [OH-].[Mg+2].[Ce+3].[OH-].[OH-].[OH-].[OH-] BYCMGBGNQBDTCB-UHFFFAOYSA-I 0.000 description 1
- FRTNIYVUDIHXPG-UHFFFAOYSA-N acetic acid;ethane-1,2-diamine Chemical class CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCN FRTNIYVUDIHXPG-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000007630 basic procedure Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- XRRONFCBYFZWTM-UHFFFAOYSA-N octadecanoic acid;sodium Chemical compound [Na].CCCCCCCCCCCCCCCCCC(O)=O XRRONFCBYFZWTM-UHFFFAOYSA-N 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 235000007686 potassium Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A kind of method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide, belongs to inorganic chemical industry technical field of material.The present invention carries out decalcification and dispersion using calcium remover and dispersant by liquid phase conversion to raw material first with calcic magnesium hydroxide as raw material, obtains dispersed high purity magnesium hydroxide；Then above-mentioned magnesium hydroxide is carried out into calcination for activation under the conditions of middle cryogenic vacuum, obtains high specific surface area porous magnesia；The above-mentioned magnesia aqueous solution of the addition containing surfactant is carried out into activating conversion again, High-purity high-activity magnesium hydroxide products are obtained.Present invention process is simple, process is gently easily-controllable, and product purity is high, specific surface area is big, activity is good, can based on inorganic chemical product or high-efficiency adsorbent be used for the fields such as medical, fire-retardant, metallurgical, catalysis, desulfurization, absorption.
Description
Technical field
The present invention relates to a kind of High-purity high-activity Preparation method of magnesium hydroxide, belong to inorganic chemical industry material preparation technology neck
Domain.
Background technology
Magnesium hydroxide is a kind of superior performance, widely used basic inorganic chemical products, wherein, High-purity high-activity hydrogen-oxygen
Change magnesium and have that impurity is few, reactivity is high because of it, high adsorption capacity the features such as, just causing people extensive as high value added product
Concern.
Preparation method of magnesium hydroxide mainly has vapor phase method and liquid phase method.Vapor phase method is general with magnesium chloride or magnesium carbonate as former
Material, prepares magnesia by roasting first, and magnesium hydroxide is then hydrolyzed into again.Such as the Aman techniques of Dead Sea group of Israel
(Harben P.Minster T.Industrial mineral development in Israel,Industrial
Minerals,1997(6),49-62.).3 covering devices are worldwide had at present using Aman technique productions magnesium hydroxides,
Including Austrian VeitsherMagresitWerke A.G. companies and Vienna Ruthner branches of Andritz companies.Aman works
Skill basic procedure：Removal of impurities treatment is carried out to extracting the bittern after potassium, sodium, bromine first, then is concentrated into magnesium chloride with high-temp waste gas
300-550g/l, is injected directly into pyrolysis in " Aman types spray reactor ", the thick magnesia of solid product after pyrolysis again through hydrolysis,
Form magnesium hydroxide.The magnesium hydroxide prepared with the method is mostly submicron order sheet products, and good dispersion, specific surface is less than
20m2/ g, is commonly used for the halogen-free flame retardants of the plastic industries such as cable.The U.S., Japan are mostly using in alkali and/or carbonate deposition halogen
Calcining manners prepare magnesia to water/seawater again, then obtain purity magnesium hydroxide higher (An Y, Yin Y, Zhang through hydrolysis
J,Zhang Y,Preparation of magnesium hydroxide used as fire retardant,by high
temperature sintering magnesite to obtain magnesium oxide,adding magnesium
oxide into deionized water,and reacting with urea to precipitate magnesium
hydroxide crystals,2012,CN102502727-A；Wang Yunshan, Xu Jingxiu, low-grade magnesite produce high-purity hydrogen-oxygen
Change magnesium and method of magnesium oxide, 2013, CN103011630A；Xue Li,Tongxin Shi,Peng Chang,Han Hu,
JiayangXie,Yunyi Liu,Preparation ofmagnesiumhydroxide flame retardant
fromlightcalcinedpowder by ammonia circulation method,Powder Technology,260
(2014)98-104；Guo Guangyuan, high purity magnesium hydroxide is prepared using Bischofite in Salt lake, chemical industry mineral and processing, and 2007, (9),
3-5)。
China typically prepares magnesium hydroxide (Yan Ya by roasting magnesite-aquation or salt lake magnesium chloride liquid phase conversion method
Alliance, the present Research of flame retardant of magnesium hydroxide, salt industry and chemical industry, 2013,42 (1), 4-7 are prepared from magnesite；Xiang Lan, Liu Feng,
Jin Yongcheng, Jin Yong, try to make a comment the height use countermeasT of China western part salt lake magnesium resource, sea lake salt and chemical industry, 2002,31 (4), 24-
27；Liu Yusheng, Liu Cui, Ma Peihua, using the technology exploration of salt lake bittern preparing magnesium hydroxide, salt lake is studied, and 2004,12 (2),
51-55).Roasting magnesite-aquation method is because raw material is containing miscellaneous more, it is difficult to obtain high purity product (Jiang Yuzhi, Han Yuexin, print ten thousand are loyal,
Bai Limei, using magnesite hydrogen manufacturing magnesia, Northeastern University's journal (natural science edition), 2006,27 (6), 694-697；Du Gao
Xiang, Wang Baikun prepares nano-grade magnesium hydroxide, ground leading edge, 2008,15 (4), 142-145 using magnesite tailings)；
Magnesium chloride liquid phase conversion method is generally with NaOH, ammoniacal liquor or calcium hydroxide etc. for magnesium chloride is converted into hydroxide by precipitating reagent
Magnesium, with process it is gentle easily-controllable the features such as, it is relatively wide (to orchid, Wu Huijun, Jin Yongcheng, Jin Yong, flame retardant type hydroxide in China's application
The commentary of magnesium technology of preparing, sea lake salt and chemical industry, 2001,30 (5), 1-4).
Liquid phase method prepares high purity magnesium hydroxide mostly with NaOH or ammoniacal liquor as precipitating reagent, product prepared by sodium-hydroxide method
It is in gel product, it is difficult to be separated by filtration more, and has sodium chlorion to adsorb hidden danger (Wu Huijun, Xiang Lan, Jin Yongcheng, Jin Yong, high dispersive
The preparation of magnesium hydrate powder and its influence factor, Journal of Inorganic Materials, 2004,19 (5), 1181-1185)；Prepared by ammonia process
Magnesium hydroxide products purity is high, be easy to filtering, but conversion per pass is low, because the operating environment that ammonia evaporation causes is poor, and by-product
Thing ammonium chloride is unmarketable, recycles (Wang Zhiqiang, Lv Bingling, Liu Jianping, Cai Ying by converting ammonia still process mode mostly at present
Thoroughbred horse, Li Fengjin, in big waves, the research of precipitation method synthesizing high pure superfine magnesium hydroxide, inorganic chemicals industry, 2001,33 (4), 3-4).
In addition, sodium-hydroxide method and ammonia process have precipitating reagent it is more expensive, it is relatively costly the problems such as.Above-mentioned technique, engineering or Technological Economy are asked
Topic limits the large-scale industrial application of sodium-hydroxide method and ammonia process.
Lime (calcium hydroxide) method production magnesium hydroxide has the easily separated feature of low cost, product, but often calcic, iron, silicon
Deng impurity, purity is generally below 97wt%, and easily reunion, activity low (Han Haibo, Zhao Hua, Liu Runjing, Hu Yongqi, Hu Qingfu, Lee
Man of virtue and ability chrysanthemum, new preparation technology of nano-sized magnesium hydroxide by lime-brine method research, inorganic chemicals industry, 2008,40 (2), 31-32).Adopt
With low solubility saturation lime solution, (Ma Zhiwei, Zhang Nanjiang, Zhou Ke, Wang Zhongchuan, Liu Huanqiang, Li Lu, bittern lime method production are high-purity
The technique of magnesium hydroxide, CN200910020974.5,2010) avoid converting admittedly, using wet screening (Zhang Yushan, yellow Xiping,
Wang Licong, Gao Chunjuan, Wang Yuqi, Cai Ronghua, the method for reducing impurity in producing magnesium hydroxide by calcium method reaction residual liquor,
CN200910070965.7,2010) remove big grain impurity, add magnesium hydroxide crystal seed (rivers and mountains, Ke Ding, Wang Zeqiang, chloride containing
Magnesium, calcium chloride mixed solution lime crystal seed method produce the method for magnesium hydroxide, CN201410025879.5,2014) induction nucleation,
Regulation and control milk of lime pH (Wang Min, Zhao has a Jing, Zhang Hongtao, Shi Lijie, Li Faqiang, Huang Peijin, a kind of method for preparing magnesium hydroxide,
CN201310632891.8,2014) slow down precipitation reaction speed, realize prepared by higher degree magnesium hydroxide.Currently for calcic
The follow-up deliming technique of reunion state magnesium hydroxide be related to it is less, using acidleach (Wang Shaoqing, Li Caihong, Liu Jinrong, using salt lake halogen
Water prepares high purity ultra-fine magnesium hydroxide, salt industry and chemical industry, 2008,37 (1), 1-4) calcic impurity can be made to enter in pickle liquor,
Reach deliming purpose.Using spinning liquid deliming method, (Hu Qingfu, Song Liying, Liu Baoshu, light burnt powder aquation legal system take flame retardant grade hydroxide
Magnesium new technology, inorganic chemicals industry, 2006,38 (7), 30-32) reach deliming purpose using density contrast.Using High-temperature water heat treatment
(monarch Wang Lan produces Flame Retardant Magnesium Hydroxide technical study, inorganic chemicals industry, 2009,41 to calcic magnesium hydroxide using bittern
(10), 42-44), promote magnesium hydroxide dissolving deposition.Can moderately improve calcic magnesium hydroxide purity, but still suffer from efficiency it is low,
Purity (generally less than 97wt%) problem not high.
Active magnesium hydroxide typically first passes through roasting magnesite-aquation method (Li Shurong, the synthesis side of active magnesium hydroxide
Method, 2008, CN101214979A), the method is that roasting magnesite first is obtained into magnesia unslacked, and magnesia unslacked is again by alkaline agent or high score
Sub- agent aquation obtains active magnesium hydroxide, and thus magnesium hydroxide specific surface area is low obtained in method, and purity is not high, or in magnesia
Surfactant (Li S, Synthesis of active magnesium hydroxide for use are added in hydration process
as adhesive involves sintering the natural magnesite,preparing
calcinedmagnesite,heating,processing emulation reaction,cooling down,and
Preparing active magnesium hydroxide solution, 2008, CN101214979-A) regulate and control its work
Property, the active magnesium hydroxide preparation technology for high-specific surface area is less,
The content of the invention
It is an object of the invention to provide a kind of process is simple, process, gently easily-controllable, added value of product is high, prepare purity
The big method for preparing High-purity high-activity magnesium hydroxide as raw material with calcic reunion state magnesium hydroxide of high, specific surface area, can conduct
Basic inorganic chemical products or high-efficiency adsorbent are used for the fields such as medical, fire-retardant, metallurgical, catalysis, desulfurization, absorption.
To realize foregoing invention target, the technical solution adopted by the present invention is as follows:
A kind of method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide, it is characterised in that method includes as follows
Step：
1) it is 5-50 microns, the calcic reunion state magnesium hydroxide of main content 85-97wt% as raw material with average aggregate particle diameter,
And calcium remover containing 0.01-20wt% and 0.01-20wt% dispersants are added, the suspension that solid holdup is 1-30wt% is made,
Reacted 0.5-36 hours at a temperature of 10-100 DEG C, filter, wash, dry, obtain dividing for the main content >=98.5wt% of magnesium hydroxide
Bulk high purity magnesium hydroxide；
2) dispersed high purity magnesium hydroxide is placed in vacuum drying oven, with 0.05-30 DEG C/minute of speed in air or nitrogen atmosphere
Degree is warming up to 300-700 DEG C, constant temperature calcining 1-24 hours, obtains specific surface area 100-800m2The porous extra light calcined magnesia of/g；
3) porous extra light calcined magnesia is added into the aqueous solution containing 0.001-20wt% surfactants, being made solid holdup is
1-40wt% suspension, then aquation is converted 0.5-10 hours at 10-150 DEG C, is filtered, washs, is dried, and obtains average original
Particle diameter 0.1-4 microns, 0.2-4 microns of average aggregate particle diameter, specific surface area be 60-500m2/ g, main content >=99wt% it is high-purity
High activity magnesium hydroxide products.
Preferably.The calcium content of described calcic reunion state magnesium hydroxide is 0.01-10wt%, average primary particle diameter is
0.1-4 microns, specific surface area be 5-40m2/g。
Preferably, the vacuum in vacuum drying oven is 10-3-104Pa。
Preferably, step 1) and 3) in drying temperature be 80-110 DEG C, drying time be 1-6 hours
In above-mentioned technical proposal, described calcium remover is tartaric acid, ethylenediamine tetra-acetic acid, sodium nitrilo triacetate, citric acid,
Glucose, carboxymethyl malonic acid and, any one or more in carboxymethyl succinic acid.
In above-mentioned technical proposal, described dispersant is sodium chloride, potassium chloride, magnesium chloride, ammonium chloride, sodium sulphate, sulfuric acid
Any one or more in potassium, magnesium sulfate, ammonium sulfate and calgon.
In above-mentioned technical proposal, described surfactant is odium stearate, AEO, CMS
Any one or more in sodium, neopelex, enuatrol, polyethylene glycol and terpenol.
The present invention proposes to prepare the magnesium hydroxide of highly crystalline high dispersive using fused salt auxiliary roasting-aquation, and the invention has
Following characteristics and high-lighting effect：1. with calcic magnesium hydroxide as raw material, first by liquid phase conversion in the normal temperature aqueous solution
Removal of impurities conversion and dispersion are carried out, decalcification purification is carried out by calcium remover, the absorption by villaumite or sulfate to magnesium hydroxide is molten
It is swollen to break hard aggregation, form purity dispersed magnesium hydroxide particle higher；2. above-mentioned magnesium hydroxide is placed in vacuum drying oven, Yu Zhong
Calcination for activation is carried out under cryogenic conditions, promotes decomposition by-products (moisture) quickly to escape by regulating and controlling vacuum, it is to avoid particle weight
Crystallization and hole fusion, obtain high specific surface area porous magnesia；3. surface is added to live in magnesia aquation conversion process
Property agent, by being adsorbed in magnesium hydroxide surface, intercept magnesium hydroxide particle recrystallization fusion in aqueous and grow up, maintain
High activity, thus prepares High-purity high-activity magnesium hydroxide products.
In a word, present invention process integrates removal of impurities, dispersion, improves activity, using calcium remover and dispersant, realizes and contains
, to the preparation of high-purity dispersion magnesium hydroxide, with process is simple, mild condition, added value of product is high for calcium reunion state magnesium hydroxide,
The advantage of efficiency high and purity (98.5wt%) high is provided simultaneously with, the magnesium hydroxide products purity prepared using the present invention is high, ratio
Surface area is big, activity is good, its can based on inorganic chemical product or high-efficiency adsorbent be used for medical, fire-retardant, metallurgical, catalysis,
The fields such as desulfurization, absorption.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Fig. 2 is raw material and its product pore size distribution figure in the embodiment of the present invention 4, and wherein curve is (a) magnesium hydroxide raw material hole
Distribution map, curve (b) is activated magnesia pore size distribution figure, and curve (c) is High-purity high-activity magnesium hydroxide products pore size distribution figure.
Specific embodiment
The invention provides a kind of method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide, with calcic hydrogen-oxygen
Change magnesium is raw material, prepares High-purity high-activity magnesium hydroxide using liquid phase removal of impurities dispersion-vacuum baking-activation hydration method, specifically
Step is as follows：
1) with calcic 0.01-10wt%, average primary particle diameter 0.1-4 microns, 5-50 microns of average aggregate particle diameter, specific surface
Product 5-40m2/ g, main content 85-97% calcic reunion state magnesium hydroxide be raw material, add calcium remover containing 0.01-20wt% with
In the aqueous solution of 0.01-20wt% dispersants, the suspension of solid holdup 1-30wt% is made, then stirs (50- at 10-100 DEG C
800 revs/min) reaction 0.5-36 hour, filtering, washing, drying (80-110 DEG C, 1-6 hours), obtain the main content of magnesium hydroxide >=
The dispersed high purity magnesium hydroxide of 98.5wt%.
2) dispersed high purity magnesium hydroxide is placed in vacuum drying oven (10-3-104Pa), with 0.05- in air or nitrogen atmosphere
30 DEG C/minute of speed are warming up to 300-700 DEG C, constant temperature calcining 1-24 hours, obtain specific surface area 100-800m2/ g's is porous high living
Property magnesia.
3) porous extra light calcined magnesia is added into the aqueous solution containing 0.001-20wt% surfactants, is made solid holdup 1-
40wt% suspension, then stirs (50-800 revs/min) aquation and converts 0.5-10 hours at 10-150 DEG C, filters, washs, dries
(80-110 DEG C, 1-6 hours), obtain average primary particle diameter 0.1-4 microns, 0.2-4 microns of average aggregate particle diameter, specific surface 60-
500m2The High-purity high-activity magnesium hydroxide products of/g, main content >=99wt%.
A kind of described method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide, described calcium remover is wine
Stone acid, ethylenediamine tetra-acetic acid, sodium nitrilo triacetate, citric acid, glucose, carboxymethyl malonic acid, carboxymethyl fourth two
Any one or more in acid；Described dispersant is sodium chloride, potassium chloride, magnesium chloride, ammonium chloride, sodium sulphate, potassium sulfate, sulphur
Any one or more in sour magnesium, ammonium sulfate, calgon；Described surfactant is odium stearate, fatty alcohol polyoxy
Any one or more in vinethene, sodium carboxymethyl starch, neopelex, enuatrol, polyethylene glycol and terpenol.
The present invention is further illustrated below by specific embodiment.
Embodiment 1
Weigh 100 grams of calcic reunion state magnesium hydroxide raw materials (calcium content 10wt%, 0.1 micron of average primary particle diameter, averagely
5 microns of aggregated particle size, specific surface area 40m2/ g, the main content 85wt% of magnesium hydroxide), addition tartaric acid containing 0.01wt%,
The aqueous solution of 20wt% sodium chloride, is made suspension containing 1wt% admittedly, is then reacted 0.5 hour in 10 DEG C of (800 revs/min) of stirrings,
Filtering, washing, dry (110 DEG C, 1 hour), obtain the dispersed high purity magnesium hydroxide of main content 98.5wt%；Dispersed is high
Pure cerium hydroxide magnesium is placed in vacuum drying oven (vacuum 10-3Pa), it is warming up to 300 DEG C, constant temperature calcining with 0.05 DEG C/minute in air atmosphere
1 hour, obtain specific surface area 800m2The porous active magnesia of/g；Above-mentioned magnesia is added into odium stearate containing 0.001wt%
The aqueous solution, be made solid holdup 1wt% suspension, 10 DEG C stir (800 revs/min) aquations convert 0.5 hour, filtering, washing,
Dry (80 DEG C, 6 hours), obtain 0.1 micron of average primary particle diameter, 0.2 micron of average aggregate particle diameter, specific surface 500m2/g, master
The High-purity high-activity magnesium hydroxide products of content 99wt%.
Embodiment 2
Weigh 100 grams of calcic reunion state magnesium hydroxide raw materials (calcium content 0.01wt%, 4 microns of average primary particle diameter, averagely
50 microns of aggregated particle size, specific surface area 5m2/ g, the main content 97wt% of magnesium hydroxide), addition ethylenediamine tetra-acetic acid containing 20wt%,
The aqueous solution of 0.01wt% potassium chloride, 5wt% calgons, is made suspension containing 30wt% admittedly, then in 100 DEG C of stirrings
(50 revs/min) are reacted 36 hours, filtering, washing, dry (80 DEG C, 6 hours), and the dispersed for obtaining main content 98.8wt% is high-purity
Magnesium hydroxide；Dispersed high purity magnesium hydroxide is placed in vacuum drying oven (vacuum 104Pa), risen with 30 DEG C/minute in nitrogen atmosphere
To 700 DEG C, constant temperature calcining 24 hours obtains specific surface area 100m to temperature2The porous active magnesia of/g；Above-mentioned magnesia is added
The aqueous solution containing 20wt% aliphatic acid polyethenoxy ethers, is made solid holdup 40wt% suspension, and (50 revs/min) are stirred at 150 DEG C
Aquation is converted 10 hours, filtering, washing, dry (80 DEG C, 6 hours), obtains 4 microns of average primary particle diameter, average aggregate particle diameter 4
Micron, specific surface 60m2The High-purity high-activity magnesium hydroxide products of/g, main content 99.8wt%.
Embodiment 3
Weigh 100 grams of calcic reunion state magnesium hydroxide raw materials (calcium content 5wt%, 2 microns of average primary particle diameter, average group
15 microns of poly- particle diameter, specific surface area 35m2/ g, the main content 92wt% of magnesium hydroxide), addition sodium nitrilo triacetate containing 10wt%,
The aqueous solution of 2wt% tartaric acid, 0.5wt% magnesium chlorides, is made suspension containing 20wt% admittedly, then stirred at 90 DEG C (450 turns/
Point) react 3 hours, filtering, washing, dry (90 DEG C, 2 hours) obtain the high-purity hydroxide of dispersed of main content 98.6wt%
Magnesium；Dispersed high purity magnesium hydroxide is placed in vacuum drying oven (vacuum 10-2Pa), it is warming up to 500 with 20 DEG C/minute in nitrogen atmosphere
DEG C, constant temperature calcining 14 hours obtains specific surface area 300m2The porous active magnesia of/g；Above-mentioned magnesia is added and is contained
The aqueous solution of 12wt% sodium carboxymethyl starches, 5wt% odium stearate, is made solid holdup 20wt% suspension, in 60 DEG C of stirrings
(350 revs/min) aquation is converted 1 hour, filtering, washing, dry (100 DEG C, 2 hours), is obtained 2 microns of average primary particle diameter, is put down
Equal 6 microns of aggregated particle size, specific surface 160m2The High-purity high-activity magnesium hydroxide products of/g, main content 99.2wt%.
Embodiment 4
Weigh 100 grams of calcic reunion state magnesium hydroxide raw materials (calcium content 2wt%, 0.5 micron of average primary particle diameter, averagely
25 microns of aggregated particle size, specific surface area 15m2/ g, the main content 95wt% of magnesium hydroxide), addition divinyl containing 5wt% four acetic acid,
1wt% carboxymethyls succinic acid, 15wt% ammonium chlorides, the aqueous solution of 2wt% potassium chloride, are made suspension containing 18wt% admittedly,
Then reacted 12 hours in 50 DEG C of (150 revs/min) of stirrings, filtering, washing, dry (95 DEG C, 4 hours) obtain main content
The dispersed high purity magnesium hydroxide of 98.9wt%；Dispersed high purity magnesium hydroxide is placed in vacuum drying oven (vacuum 50Pa), in sky
Atmosphere is warming up to 400 DEG C in enclosing with 10 DEG C/minute, and constant temperature calcining 4 hours obtains specific surface area 200m2The porous active oxidation of/g
Magnesium；Above-mentioned magnesia is added the aqueous solution of neopelex containing 10wt%, 2wt% stearic acid sodium, solid holdup is made
25wt% suspension, stirs (650 revs/min) aquation and converts 8 hours at 120 DEG C, filtering, washing, dry (105 DEG C, 5 hours),
Obtain 0.5 micron of average primary particle diameter, 3 microns of average aggregate particle diameter, specific surface 360m2/ g, main content 99.6wt% it is high-purity
High activity magnesium hydroxide products.
Embodiment 5
Weigh 100 grams of calcic reunion state magnesium hydroxide raw materials (calcium content 2wt%, 1.5 microns of average primary particle diameter, averagely
32 microns of aggregated particle size, specific surface area 33m2/ g, the main content 96.5wt% of magnesium hydroxide), addition citric acid containing 1.8wt%,
2wt% ethylenediamine tetra-acetic acids, 4.5wt% sodium sulphate, the aqueous solution of 6wt% magnesium chlorides, are made suspension containing 12wt% admittedly, then
Reacted 24 hours in 30 DEG C of (100 revs/min) of stirrings, filtering, washing, dry (95 DEG C, 4 hours) obtain main content 99.1wt%
Dispersed high purity magnesium hydroxide；Dispersed high purity magnesium hydroxide is placed in vacuum drying oven (vacuum 102Pa), in air atmosphere
450 DEG C are warming up to 12 DEG C/minute, constant temperature calcining 16 hours obtains specific surface area 600m2The porous active magnesia of/g；Will be upper
State magnesia and add enuatrol containing 0.02wt%, the aqueous solution of 8wt% polyethylene glycol, be made solid holdup 30wt% suspension,
90 DEG C of stirring (150 revs/min) aquations are converted 4 hours, and filtering, washing, dry (100 DEG C, 3 hours) obtain average primary particle diameter
1.5 microns, 3.5 microns of average aggregate particle diameter, specific surface 280m2The High-purity high-activity magnesium hydroxide of/g, main content 99.4wt%
Product.
Embodiment 6
Weigh 100 grams of calcic reunion state magnesium hydroxide raw materials (calcium content 6wt%, 1 micron of average primary particle diameter, average group
6 microns of poly- particle diameter, specific surface area 28m2/ g, the main content 90wt% of magnesium hydroxide), add glucose containing 0.8wt%, 7wt% wine
Stone acid, the aqueous solution of 20wt% potassium sulfates, are made suspension containing 5wt% admittedly, then in (350 revs/min) reactions 30 of 80 DEG C of stirrings
Hour, filtering, washing, dry (95 DEG C, 4 hours) obtain the dispersed high purity magnesium hydroxide of main content 98.6wt%；Will dispersion
Shape high purity magnesium hydroxide is placed in vacuum drying oven (vacuum 10-2Pa), it is warming up to 320 DEG C, constant temperature roasting with 2 DEG C/minute in nitrogen atmosphere
Burn 6 hours, obtain specific surface area 700m2The porous active magnesia of/g；Above-mentioned magnesia is added containing 1wt% polyethylene glycol
The aqueous solution, is made solid holdup 10wt% suspension, and stirring (200 revs/min) aquation at 100 DEG C converts 5 hours, filters, washs, does
Dry (105 DEG C, 5 hours), obtain 1 micron of average primary particle diameter, 3 microns of average aggregate particle diameter, specific surface 300m2/ g, main content
The High-purity high-activity magnesium hydroxide products of 99.2wt%.
Embodiment 7
Weigh 100 grams of calcic reunion state magnesium hydroxide raw materials (calcium content 1wt%, 0.3 micron of average primary particle diameter, averagely
10 microns of aggregated particle size, specific surface area 45m2/ g, the main content 96.8wt% of magnesium hydroxide), add carboxymethyl containing 5wt% third
Diacid, the acetic acid of 12wt% divinyls four, 10wt% magnesium sulfate, the aqueous solution of 1wt% ammonium sulfate, are made and are suspended containing 16wt% admittedly
Liquid, then reacts 10 hours in 40 DEG C of (200 revs/min) of stirrings, and filtering, washing, dry (95 DEG C, 6 hours) obtain main content
The dispersed high purity magnesium hydroxide of 98.8wt%；Dispersed high purity magnesium hydroxide is placed in vacuum drying oven (vacuum 50Pa), in nitrogen
Atmosphere is warming up to 400 DEG C in enclosing with 16 DEG C/minute, and constant temperature calcining 14 hours obtains specific surface area 300m2The porous active oxidation of/g
Magnesium；Above-mentioned magnesia is added into the aqueous solution containing 12wt% terpenols, solid holdup 25wt% suspension is made, in 80 DEG C of stirrings
(300 revs/min) aquation convert 8 hours, filtering, washing, dry (105 DEG C, 2 hours), obtain 0.3 micron of average primary particle diameter,
2 microns of average aggregate particle diameter, specific surface 250m2The High-purity high-activity magnesium hydroxide products of/g, main content 99.9wt%.
Embodiment 8
Weigh 100 grams of calcic reunion state magnesium hydroxide raw materials (calcium content 4wt%, 1.5 microns of average primary particle diameter, averagely
20 microns of aggregated particle size, specific surface area 32m2/ g, the main content 94wt% of magnesium hydroxide), add carboxymethyl containing 10wt% third
Diacid, 2wt% citric acids, 10wt% ammonium sulfate, the aqueous solution of 2wt% calgons, are made suspension containing 15wt% admittedly, so
Reacted 5 hours in 60 DEG C of (250 revs/min) of stirrings afterwards, filtering, washing, dry (90 DEG C, 4 hours) obtain main content 98.7wt%
Dispersed high purity magnesium hydroxide；Dispersed high purity magnesium hydroxide is placed in vacuum drying oven (vacuum 103Pa), in air atmosphere
550 DEG C are warming up to 20 DEG C/minute, constant temperature calcining 14 hours obtains specific surface area 500m2The porous active magnesia of/g；Will be upper
State magnesia and add enuatrol containing 5wt%, the aqueous solution of 2wt% neopelexes, be made solid holdup 12wt% suspensions
Liquid, stirs (200 revs/min) aquation and converts 2 hours at 130 DEG C, and filtering, washing, dry (105 DEG C, 6 hours) obtain average original
1.5 microns of beginning particle diameter, 2.5 microns of average aggregate particle diameter, specific surface 400m2The High-purity high-activity hydrogen of/g, main content 99.5wt%
Magnesium oxide product.
Claims (4)
1. a kind of method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide, it is characterised in that method includes following step
Suddenly：
1) it is 5-50 microns, the calcic reunion state magnesium hydroxide of main content 85-97wt% as raw material with average aggregate particle diameter, and adds
Enter calcium remover containing 0.01-20wt% and 0.01-20wt% dispersants, the suspension that solid holdup is 1-30wt% is made, in 10-
Reacted 0.5-36 hours at a temperature of 100 DEG C, filter, wash, dry, obtain the dispersed of the main content >=98.5wt% of magnesium hydroxide
High purity magnesium hydroxide；The calcium content of described calcic reunion state magnesium hydroxide is 0.01-10wt%, average primary particle diameter is 0.1-
4 microns, specific surface area be 5-40m2/g；Described calcium remover is tartaric acid, ethylenediamine tetra-acetic acid, sodium nitrilo triacetate, lemon
Any one or more in acid, glucose, carboxymethyl malonic acid, carboxymethyl succinic acid；Described dispersant is chlorine
Change in sodium, potassium chloride, magnesium chloride, ammonium chloride, sodium sulphate, potassium sulfate, magnesium sulfate, ammonium sulfate and calgon any one or
It is various；
2) dispersed high purity magnesium hydroxide is placed in vacuum drying oven, with 0.05-30 DEG C/minute of speed liter in air or nitrogen atmosphere
Temperature obtains specific surface area 100-800m to 300-700 DEG C, constant temperature calcining 1-24 hours2The porous extra light calcined magnesia of/g；
3) porous extra light calcined magnesia is added into the aqueous solution containing 0.001-20wt% surfactants, is made solid holdup for 1-
40wt% suspension, then aquation is converted 0.5-10 hours at 10-150 DEG C, is filtered, washs, is dried, and obtains average original grain
Footpath 0.1-4 microns, 0.2-4 microns of average aggregate particle diameter, specific surface area be 60-500m2/ g, main content >=99wt% it is high-purity high
Active magnesium hydroxide products.
2. a kind of method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide according to claim 1, it is special
Levy and be：Vacuum in vacuum drying oven is 10-3-104Pa。
3. a kind of method that High-purity high-activity magnesium hydroxide is prepared by calcic magnesium hydroxide according to claim 1, it is special
Levy and be：Step 1) and 3) in drying temperature be 80-110 DEG C, drying time be 1-6 hours.
4. a kind of by calcic magnesium hydroxide preparation High-purity high-activity hydroxide according to claim 1-3 any claims
The method of magnesium, it is characterised in that：Described surfactant be odium stearate, AEO, sodium carboxymethyl starch,
Any one or more in neopelex, enuatrol, polyethylene glycol and terpenol.
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| CN105734331A (en) * | 2016-05-05 | 2016-07-06 | 北京交通大学 | Aluminum alloy calcium remover as well as preparation method and use method thereof |
| CN107739042B (en) * | 2017-11-22 | 2019-09-17 | 中国科学院青海盐湖研究所 | The method that high-purity magnesium sulfate is prepared by magnesium sulfate waste |
| CN108726543A (en) * | 2018-07-06 | 2018-11-02 | 中国核动力研究设计院 | A kind of simple dispersing method of magnesium hydroxide |
| CN111439765B (en) * | 2020-04-15 | 2023-02-28 | 山东格润德环保科技有限公司 | Decalcification method for producing magnesium hydroxide suspension and application thereof |
| CN111450724B (en) * | 2020-04-15 | 2022-05-03 | 山东格润德环保科技有限公司 | Magnesium hydroxide suspension with low impurity content and preparation method thereof |
| CN112174193A (en) * | 2020-10-21 | 2021-01-05 | 武汉工程大学 | Preparation method of monodisperse nano ITO |
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